......DE..........................................
R
0668613
EUROPEAN PATENT APPLICATION
published in accordance with Art. 158(3) EPC
A1
19950823
EP
94928219.8
19940902
ru
en
en
6420193
19930909
BY
19950823
199534
19950823
199534
6
6H 01L 21/66 A
de
METHODE ZUR BESTIMMUNG DER SAUERSTOFFKONZENTRATION IN SILIZIUMKRISTALLEN
en
METHOD OF DETERMINING THE CONCENTRATION OF OXYGEN IN SILICON CRYSTALS
fr
PROCEDE DE DETERMINATION DE LA CONCENTRATION D'OXYGENE DANS DES CRISTAUX DE SILICIUM
SOVIET-GERMAN JOINT VENTURE "MAMT"
01930600
FB 5435/G8548EP
"MAMT", SOVIET-GERMAN JOINT VENTURE
ul. Olesheva, 14
Minsk 220090
BY
LITVINOV, Valentin Vladimirovich
ul. Lynkova, 29-1-25
Minsk, 220128
BY
POKATILO, Jury Mifodievich
pr. Pavdy, 14-164
Minsk, 220116
BY
URINEV, Valery Ivanovich
ul. R. Luxemburg, 111a-32
Minsk, 220036
BY
Symes, Christopher A.
et al
00047961
FORRESTER & BOEHMERT Franz-Joseph-Strasse 38
80801 München
DE
DE
BY9400001
19940902
ru
WO9507546
19950316
199512
The proposed method of determining the oxygen content of silicon crystals relates to electronics and can be used for sorting silicon crystals according to their oxygen content and also for optimizing crystal production techniques based on the Chokh- ralski method. In essence, the method involves: generation of three alternate beams of radiation of different wavelengths, one of which lies at the absorption maximum of interstitial oxygen at 5.81 µm, the other two being outside its limits in a region of linear spectral dependence of the background optical density of the crystal; using monochromatic radiation from a three-wavelength CO laser with a modulating disk incorporated into the resonator, the said disk alternately switching one of the beans on and off; measuring two ratios of radiation transmission coefficients of the crystal, while the oxygen concentration being sought is determined with the aid of an established function.

Field
The invention relates to electronics and can be used for control of content and distribution of oxygen in silicon ingots.

Prior Art
There is known a conventional optic method of determining the concentration of oxygen in silicon (Certificate of Authorship of the USSR No. 1447201, cl. H 01 L 21/66, 1986), based on the determining the coefficient of absorption at the absorption maximum of 5.8 µm.
The disadvantage of this conventional method is the necessity of separating the ingots into wafers and optically polishing their surfaces.
There is also known a method of controlling oxygen distribution in silicon ingots along the aids of their growth (Certificate of Authorship of the USSR No. 1669340, cl. H 01 L 21/66, 1991) involving irradiating an unpolished side of the ingot under examination with three beams of IR-radiation, two of which beams having different wavelengths outside the absorption band and the third beam having a wavelength of 5.81 µm (1720cm-^1), corresponding to a range of interstitial oxygen absorption. Detection of the incident and transmitted radiation intensities and subsequent determination of the transmission coefficients, enables the oxygen concentration to be determined by reference to known values.
However, the application of the above method for control of industrial ingots, being products grown according to the Czochralski method and having an oxygen concentration of more than 2 x 10^{17}cm^{-3}, is insufficiently sensitive, requires chemical etching of the ingot surfaces, and gives insufficiently localised measurements.

Disclosure of the Invention
It is an object of this invention to increase the precision and locality control of oxygen distribution in silicon ingots.
The essence of the invention is determining the silicon ingot oxygen concentration by irradiating the ingot with three alternating beams of IR-radiation of different wavelengths, one of which wavelengths lies at the absorption maximum of interstitial oxygen, 5.81 µm, the other two being outside the absorption band According to the present invention the ingots are exposed to three monochromatic beams of radiation from a three wavelength CO laser with a modulating disk incorporated into the resonator, which disk sequentially switches the generation of each one of the beams on and off. Two ratios of radiation transmission coefficients are then measured, and the required oxygen concentration is determined according to the formula:wherein K = 2 x 10^{19}cm^{-2}- calibration coefficient. d - ingot thickness.- a coefficient, defined by selection of analytical wavelengths.
λ_1, \_3 - the wavelengths outside the absorption band.
X_2 - wavelength corresponding to absorption maximum.
Ti, T_2, T_3 - transmission coefficients at wavelengths λ_1, x_2, X_3 respectively.
The claimed technical solution differs from the prior art in that it uses monochromatic beams of radiation, produced by interresonator modulation of generation of a three wavelength CO laser with a rotating modulating disk to determine two ratios of radiation transmission coefficients of the ingot.

Brief Description of Drawings
- Figure 1 shows the variation of the measured absorption coefficient (a_{meas}) determined at 5.81 µm, with interstitial oxygen concentration (N) detected according to the prior art (1) and the proposed method (2).
- Figure 2 shows an optical scheme of the three wavelength CO laser with a modulating disk incorporated into the resonator, wherein 1 is a discharge tube, 2 is a non-transmitting mirror, 3 is a defrac- tion grating, 4, 5, 6 are auxiliary mirrors and 7 is a modulating disk.
- Figure 3 shows the spectral dependency of background optical density (In 1/T) for a P-type silicon ingot with a specific resistance of 12 9 cm for different types of surface, where 1 - optical polishing, 2 - chemical etching, 3 - lapped diffusing surface.
- Figure 4 shows radial oxygen distribution in silicon ingots with 100 mm diameter and 95mm length.
- Figure 5 shows an oxygen distribution profile along the axis of growth of an ingot having a diameter of 150mm.

Preferred Embodiment
The method is as follows.
Three beams of monochromatic radiation of a three wavelength CO laser are alternately passed through the cylindrical ingot being examined, falling parallel or perpendicular to the aids of ingot growth, one of which beams has the wavelength X_2 = 5.81µm corresponding to the absorption maximum of oxygen, and the other two beams have wavelengths, λ_1, X_3 outside the absorption band in a region of linear spectral dependence of the background optical density of the ingot (Figure 3). The two ratios Of intensity of incident radiation 1_0 (λ_1)/l_o-(x2), l_o (λ_1 )/l(λ_3) and transmitted radiation I(λ_1 )/(X_2), I (λ_1)/I(λ_3) are determined by means of two photodetectors, an amplifier, a digitizer and a micro-computer. After that the oxygen concentration being sought in the irradiated part of the ingot is determined according to the formulawhere K = 2x10^{19} cm-^{2 -} is a calibrating coefficient; d - ingot thickness,coefficient defined by selection of analytical wavelengths, andare radiation transmission coefficients at the three wavelengths λ_1, x_2, X_3 respectively.
If equality of incident beam intensity is obtained by means of regulating the diameter of the modulating disk orifices such that l_o (λ_1) = l_o(λ_2) = l_o (λ_3), only the transmitted beam intensities are detected and the second photodetector is no longer necessary.
Another embodiment of this method is based on separation of the laser beams into two parts by means of a separating plate, one of which parts is passed through the crystal having a thickess where the oxygen content is known (the reference crystal). By means of one or two photodetectors, the ratios of intensity of radiation beams transmitted by the crystal being examined I(λ_1)/I(λ_2), I(λ_1)/I(λ_3) and reference crystal l_o (λ_1 )/l_o(λ_2), l_o (λ_1 )/l_o(λ_3) may be determined, and according to the foregoing formula the difference in the oxygen concentration in the examined and reference ingots is determined.
The results of this embodiment for determining the longitudinal and lateral distribution of oxygen in industrial silicon ingots are shown in Figure 4 and Figure 5.

Industrial Application
The present invention, a method of determining the oxygen concentration in silicon crystals, may be widely utilised in electronics and other industries for control of the content and distribution of oxygen in silicon ingots.
The invention may also be used for sorting silicon ingots or parts thereof according to their oxygen content ratios before cutting into industrial wafers, as well as in developing the technology of growing homogeneous silicon ingots.
1. A method of determining the concentration of oxygen in silicon crystals, involving alternately passing through the ingot three IR-radiation beams having different wavelengths, one of which wavelengths lies at the absorption maximum of interstitial oxygen at 5.81 µm, the other two being out of the absorption band. The method is different from the prior art in that the ingots are exposed to three monochromatic radiation beams from a three-wavelength CO laser with a modulating disk incorporated into a resonator, which disk alternately switches each one of the beams on and off. Two ratios of radiation transmission coefficients of the ingot are measured, while the oxygen concentration being sought is determined according to the following formula:wherein K = 2 x 10^{19}cm^{-2}- is a calibration coefficient, d - ingot thickness,- coefficient, defined by selection of analytical wavelength,
λ_1, λ_3- wavelength outside the absorption band. λ_2- wavelength corresponding to maximum absorption band,
Ti, T_2, T_3 - transmission coefficients values at wavelengths λ_1, λ_2, X_3 respectively.